巯基聚倍半硅氧烷合成的影响因素

Influence factors of mercapto polysilsesquioxane synthesis

以巯丙基三甲氧基硅烷为原料,在甲醇作溶剂、浓HCl作催化剂的条件下水解缩合制备了巯基聚倍半硅氧烷,并用红外光谱和凝胶色谱对其进行了表征,通过折光率和产率的测定研究了溶剂、水量、反应温度、反应时间和催化剂用量对产物性能的影响。结果表明,60℃下以甲醇为溶剂,p H=2.0,原料与水物质的量比1∶3,单体与溶剂质量比1∶1,水解缩合反应8 h,产率达90%以上。

The mercapto polysilsesquioxane was synthesized by hydrolytic condensation using mercapto propyl trimethoxysilane(KH-590) as raw material,methanol as solvent and concentrated hydrochloric acid as catalyst. The product structure were characterized by FTIR and GPC. The effects of solvents,water amount,reaction temperature,reaction time and the catalyst amount on the product properties were investigated by the determination of refractive index and yield. The results showed that the optimum conditions were as followed:methanol as solvent,p H = 2.0,molar ratio of mercapto monomer to water 1 ∶ 3,mass ratio of solvent to monomer 1 ∶ 1,reaction temperature 60 ℃ and reaction time 8 h. The yield of the product was up to 90%.